HRID1244726

反应详情

EQUATION

反应方程式

HRID 1244726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Cis-1-[(1,1-dimethylethoxy)carbonylamino]-2-methanesulphonyloxyindan (18.1 g, 55.3 mmol) was dissolved in dry dimethyl acetamide (100 ml). Sodium azide (5.4 g, 83.0 mmol) was added and the mixture heated to 90° C. for 6 hours. The reaction was cooled, diluted with ethyl acetate (150 ml), washed with water (6×200 ml) and dried over magnesium sulphate. 10% Palladium on activated carbon was added and the mixture stirred under a hydrogen atmosphere for 24 hours. Filtration through celite followed by evaporation gave the title compound (2.6 g, 98%) as a white solid.

WORKUP

后处理

  1. temperatureThe reaction was cooled
  2. washwashed with water (6×200 ml)
  3. dry with materialdried over magnesium sulphate
  4. addition10% Palladium on activated carbon was added
  5. filtrationFiltration through celite
  6. customfollowed by evaporation